CN105985765B - Fracturing fluid thickener and preparation method thereof and fracturing fluid - Google Patents
Fracturing fluid thickener and preparation method thereof and fracturing fluid Download PDFInfo
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Abstract
A kind of fracturing fluid thickener of present invention offer and preparation method thereof and fracturing fluid, the fracturing fluid thickener group become：Acrylamide, unsaturated carboxylic acid, alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N dimethyl alkyl tertiary amines, halogenated cyclic ethers, initiator and water, wherein, the acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, the sum of mass percent of N dimethyl alkyl tertiary amine and the halogenated cyclic ethers is 15%~25%, the mass percent of the initiator is 0.04%~0.09%, fracturing fluid thickener provided by the invention, when solving in the prior art using guanidine glue and its modifier as the thickener of fracturing fluid due to guanidine glue and its easy corruption of modifier cause to return drain intractability after breaking gel it is big, it is of high cost, the technical issues of reusing poor feasibility.
Description
Technical field
The present invention relates to a kind of oil gas field auxiliary agent technical field, more particularly to a kind of overall process takes the low frictional resistance slippery water of sand
Fracturing fluid thickener and preparation method thereof and fracturing fluid.
Background technology
Pressure break is one of Main Yield-increasing measure of Low permeable oil and gas reservoirs, is to utilize hydraulic action, oil-gas Layer is made to form crack
A kind of method, also known as oil-gas Layer hydraulic fracturing, oil-gas Layer fracturing technology process be use fracturing unit truck, high-pressure large-displacement have one
The liquid for determining viscosity squeezes into oil-gas Layer, after oil-gas Layer is extruded many cracks, proppant (such as quartz sand) is added and is filled in
The penetrating power of oil-gas Layer is improved in crack, to increase water injection rate (water injection well) or oil production (oil well), in fracturing process, and note
Enter the liquid in well and be referred to as fracturing fluid, fracturing fluid is the important component of fracturing technique, is generally wanted to the performance of fracturing fluid
It asks：Viscosity is high, and lubricity is good, and filter loss is small, pollution-free to fluid mine to without blocking and being damaged by the fluid layer of pressure break, generally
Fracturing fluid has the types such as aqueous fracturing fluid, oil base fracturing fluid, emulsus fracturing fluid, foam fracturing fluid and acid-base fracturing fluid.
Currently, common fracturing fluid is mainly the fracturing fluid using guanidine glue and its modifier as the aqueous fracturing fluid of thickening agent
It is widely applied in each oil gas field, and achieves good effect of increasing production, but oil gas field " batch production " pressure break is celebrated with long
The it is proposed of work pattern and Environmental Protection Situation are increasingly severe, it is desirable that aqueous fracturing fluid in addition to Low Damage, low frictional resistance, low cost,
Except the easy row of returning, easy continuous mixture feature, also there is the characteristics of easily recycling, high recycling rate, drain is returned after being pressed with reduction
The amount of conserving water while to environment and soil pollution.
However when using guanidine glue and its modifier as the thickening agent of fracturing fluid, guanidine glue and its modifier have natural plant gum perishable
The shortcomings that losing, after frozen glue is formed by chemical crosslinking, it is big to return drain intractability after breaking gel, of high cost, reuses feasibility
Difference, so environmental protection pressure cannot be alleviated when using guanidine glue and its modifier as the thickening agent of fracturing fluid and cannot be satisfied " batch production "
Construction requirement.
Invention content
The present invention provides a kind of fracturing fluid thickener, solves in the prior art using guanidine glue and its modifier as fracturing fluid
Thickener when due to big, of high cost, the recycling that causes to return drain intractability after breaking gel of guanidine glue and its easy corruption of modifier
The technical issues of poor feasibility.
It is easy to operate easily controllable in preparation process the present invention also provides a kind of preparation method of fracturing fluid thickener, system
Fracturing fluid thickener is not corrupt made of standby, heat-resistant salt-resistant, rises glue soon in water, meets continuous mixture requirement, which increases
Thick dose has good Efficient Adhesive Promotion, and adjust it in due course just can realize that drop blocks water and load fluid function using concentration.
The present invention provides a kind of fracturing fluid, which includes the fracturing fluid thickener of above-mentioned preparation, pressure break when application
Liquid returns that drain treatment process is simple, flowback effect is preferable, cost is relatively low, high recycling rate, while alleviating environmentally friendly pressure break
The requirement of " batch production " fracturing work can be met very well.
The present invention provides a kind of fracturing fluid thickener, and the fracturing fluid thickener group becomes：Acrylamide, unsaturated carboxylic
Acid, alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine, halogenated cyclic ethers, initiator and water, wherein described
Acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine
It is 15%~25% with the sum of the mass percent of the halogenated cyclic ethers, the mass percent of the initiator is 0.04%~
0.09%.
In fracturing fluid thickener provided by the invention, the fracturing fluid thickener is by acrylamide, unsaturated carboxylic acid, alkyl phenol
Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers, initiator and water composition, wherein the propylene
Amide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and institute
It is 15%~25%, i.e. acrylamide to state the sum of mass percent that five components of halogenated cyclic ethers account in fracturing fluid thickener
Mass percent, the mass percent of unsaturated carboxylic acid, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- bis-
The sum of the mass percent of methyl-alkyl tertiary amine and the mass percent of halogenated cyclic ethers are 15%~25%, such as acrylamide
Mass percent can be 5%, the mass percent of unsaturated carboxylic acid can be 5%, alkyl phenol Polyoxyalkylene ethers unsaturated acids
The mass percent of ester can be 3%, N, and the mass percent of N- dimethyl-alkyl tertiary amine can be 3%, the matter of halogenated cyclic ethers
Amount percentage can be 3% or the mass percent of acrylamide can be 8%, the mass percent of unsaturated carboxylic acid can
Think 8%, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester can be 5%, N, the matter of N- dimethyl-alkyl tertiary amine
It can be 2% to measure percentage, and the mass percent of halogenated cyclic ethers can be 2%, in the present invention, as long as the quality hundred of acrylamide
Divide ratio, the mass percent of unsaturated carboxylic acid, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-
The sum of the mass percent of alkyl tertiary amine and the mass percent of halogenated cyclic ethers in the range of 15%~25%, acrylamide
Mass percent, the mass percent of unsaturated carboxylic acid, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- bis-
The mass percent of methyl-alkyl tertiary amine and the mass percent of halogenated cyclic ethers can be in any combination.
Also include initiator in the present invention, initiator is that one kind is easy to be thermally decomposed into free radical (i.e. primary group of free radicals)
Compound, can be used for cause alkenes, double vinyl monomers free radical polymerization and copolymerization, it can also be used to unsaturated polyester (UP)
Crosslinking curing and high molecular crosslink reaction, the present invention in, by include initiator cause acrylamide, unsaturated carboxylic acid, alkane
Base phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers carry out reaction and increase to which fracturing fluid be made
Thick dose, in the present invention, the mass percent of initiator is 0.04%~0.09%, for example, the mass percent of initiator can be with
It is 0.06% or 0.08%, can also be for 0.09%, in the present invention, fracturing fluid thickener is to make dispersion with water to be situated between
Matter, so, when the mass percent of acrylamide, the mass percent of unsaturated carboxylic acid, alkyl phenol Polyoxyalkylene ethers are unsaturated
The mass percent of acid esters, N, the mass percent of N- dimethyl-alkyl tertiary amine and the sum of the mass percent of halogenated cyclic ethers are
15%~25%, when the mass percent of initiator is 0.04%~0.09%, remaining mass percent is the quality hundred of water
Divide ratio.
In the concrete scheme of the present invention, the acrylamide, the unsaturated carboxylic acid, the alkyl phenol polyoxy alkene
The sum of mass percent of ether unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers be 15%~
25%, and the acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- diformazans
The molar ratio of base-alkyl tertiary amine and the halogenated cyclic ethers is 99：25：1：1：1, that is, the acryloyl in fracturing fluid thickener
Amine, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and described
Halogenated cyclic ethers is 99 according to molar ratio：25：1：1：1 mixing, and after mixing, it is the acrylamide, the unsaturated carboxylic acid, described
The mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers it
Be 15%~25%.
In the concrete scheme of the present invention, the initiator includes but not limited to by ammonium persulfate and potassium thiosulfate
Composition, and the molar ratio of the ammonium sulfate and the potassium thiosulfate is 1：1, in of the invention, the initiator can also be by mistake
Potassium sulfate and sodium hydrogensulfite composition, the potassium peroxydisulfate and sodium hydrogensulfite are 1 according to molar ratio：1 measures, wherein when drawing
When hair agent is potassium peroxydisulfate and sodium hydrogensulfite, the addition manner of initiator is first to add the potassium peroxydisulfate, is added again after 5min
Add the sodium hydrogensulfite, in of the invention, when initiator is made of ammonium persulfate and potassium thiosulfate, the addition manner of initiator
Ammonium persulfate can be first added, adds potassium thiosulfate after 5min again, or simultaneously add ammonium persulfate and potassium thiosulfate.
In the concrete scheme of the present invention, in specific embodiments of the present invention, by acrylamide, unsaturated carboxylic
Acid, alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, it is described when N- dimethyl-alkyl tertiary amine, the reaction of halogenated cyclic ethers generate thickener
Unsaturated carboxylic acid can be one or more in acrylic acid, butenoic acid or metal acid-salt, and wherein acrylic acid can be straight chain
Acrylic acid can also be the acrylic acid with branch, and butenoic acid can be the butenoic acid of straight chain, can also be the fourth with branch
Olefin(e) acid, atomic number of alkyl carbon can be 7,8 or 12 in the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the alkyl phenol polyoxy alkene
Polyoxyalkylene ethers can be polyoxyethylene ether or polyethenoxy ether, the alkyl phenol Polyoxyalkylene ethers unsaturated acids in ether unsaturated acid ester
Unsaturated acid ester can be acrylate or butenoate in ester, and wherein acrylate can be the acrylate of straight chain, may be used also
Think that the acrylate with branch, butenoate can be the butenoate of straight chain, can also be the butenoic acid with branch
Ester；Atomic number of alkyl carbon is alkyl in 6-18, such as N, N- dimethyl-alkyl tertiary amine in the N, N- dimethyl-alkyl tertiary amine
Carbon atom number can be 8,9 or 12；Halo groups are fluorine, chlorine or bromine in the halogenated cyclic ethers, such as can be fluoro cyclic ethers, can
Think chloro cyclic ethers, can also be bromo cyclic ethers, suitable unsaturated carboxylic acid, alkyl phenol polyoxy are chosen with specific reference to practical application
Alkene ether unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine, halogenated cyclic ethers generate thickener.
The present invention also provides the preparation methods of above-mentioned fracturing fluid thickener, including following procedure：
Unsaturated carboxylic acid is dissolved in water, adjustment pH is 7, and water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, acrylamide and alkyl phenol Polyoxyalkylene ethers unsaturated acid ester stirring and dissolving is added；
Initiator is added, N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers are added after reacting 1h, reaction time 6-8h,
The fracturing fluid thickener is made, wherein
The acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- diformazans
The sum of mass fraction of base-alkyl tertiary amine and the halogenated cyclic ethers be 15~25, the initiator quality number be 0.04~
0.09, surplus is water.
In the present invention, unsaturated carboxylic acid is dissolved in water, the pH that solution is adjusted with potassium hydroxide is 7, by reaction liquid
Water bath with thermostatic control is to 35 DEG C, and then under conditions of maintaining nitrogen purge, acrylamide and alkyl phenol Polyoxyalkylene ethers unsaturated acids is added
Ester stirring and dissolving adds initiator, and N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers are continuously added after reacting 1h, continues anti-
Fracturing fluid thickener is made after answering 8-10 hours.
In fracturing fluid thickener prepared by the present invention, the fracturing fluid thickener is by acrylamide, unsaturated carboxylic acid, alkyl phenol
Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers, initiator and water, wherein the acrylamide,
The unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and described halogenated
The sum of mass fraction that five components of cyclic ethers account in fracturing fluid thickener be 15~25, i.e., the mass percent of acrylamide,
The mass percent of unsaturated carboxylic acid, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tert
The sum of the mass percent of amine and the mass percent of halogenated cyclic ethers be 15%~25%, such as such as acrylamide quality hundred
Divide than that can be 5%, the mass percent of unsaturated carboxylic acid can be 5%, the quality of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester
Percentage can be 3%, N, and the mass percent of N- dimethyl-alkyl tertiary amine can be 3%, the mass percent of halogenated cyclic ethers
Can be 3% or the mass percent of acrylamide can be 8%, the mass percent of unsaturated carboxylic acid can be 8%,
The mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester can be 5%, N, the mass percent of N- dimethyl-alkyl tertiary amine
Can be 2%, the mass percent of halogenated cyclic ethers can be 2%, in the present invention, as long as the mass percent of acrylamide, no
The mass percent of saturated carboxylic acid, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine
Mass percent and halogenated cyclic ethers the sum of mass percent in the range of 15%~25%, the quality percentage of acrylamide
Than, the mass percent of unsaturated carboxylic acid, the mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkane
The mass percent of base tertiary amine and the mass percent of halogenated cyclic ethers can be in any combination.
Also include initiator in the present invention, initiator is that one kind is easy to be thermally decomposed into free radical (i.e. primary group of free radicals)
Compound, can be used for cause alkenes, double vinyl monomers free radical polymerization and copolymerization, it can also be used to unsaturated polyester (UP)
Crosslinking curing and high molecular crosslink reaction, the present invention in, by include initiator cause acrylamide, unsaturated carboxylic acid, alkane
Base phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers carry out reaction and increase to which fracturing fluid be made
Thick dose, in the present invention, the mass percent of initiator is 0.04%~0.09%, for example, the mass percent of initiator can be with
It is 0.06% or 0.08%, can also be for 0.09%, in the present invention, fracturing fluid thickener is to make dispersion with water to be situated between
Matter, so, when the mass percent of acrylamide, the mass percent of unsaturated carboxylic acid, alkyl phenol Polyoxyalkylene ethers are unsaturated
The mass percent of acid esters, N, the mass percent of N- dimethyl-alkyl tertiary amine and the sum of the mass percent of halogenated cyclic ethers are
15%~25%, when the mass percent of initiator is 0.04%~0.09%, remaining mass percent is the quality hundred of water
Divide ratio.
In the concrete scheme of the present invention, the acrylamide, the unsaturated carboxylic acid, the alkyl phenol polyoxy alkene
The sum of mass percent of ether unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers be 15%~
25%, and the acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- diformazans
The molar ratio of base-alkyl tertiary amine and the halogenated cyclic ethers is 99：25：1：1：1, that is, the acryloyl in fracturing fluid thickener
Amine, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and described
Halogenated cyclic ethers is 99 according to molar ratio：25：1：1：1 mixing, and after mixing, it is the acrylamide, the unsaturated carboxylic acid, described
The mass percent of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers it
Be 15%~25%.
In the concrete scheme of the present invention, the initiator includes but not limited to by ammonium persulfate and potassium thiosulfate
Composition, and the molar ratio of the ammonium sulfate and the potassium thiosulfate is 1：1, in of the invention, the initiator can also be by mistake
Potassium sulfate and sodium hydrogensulfite composition, the potassium peroxydisulfate and sodium hydrogensulfite are 1 according to molar ratio：1 measures, wherein when drawing
When hair agent is potassium peroxydisulfate and sodium hydrogensulfite, the addition manner of initiator is first to add the potassium peroxydisulfate, is added again after 5min
Add the sodium hydrogensulfite, in of the invention, when initiator is made of ammonium persulfate and potassium thiosulfate, the addition manner of initiator
Ammonium persulfate can be first added, adds potassium thiosulfate after 5min again, or simultaneously add ammonium persulfate and potassium thiosulfate.
In the concrete scheme of the present invention, in specific embodiments of the present invention, by acrylamide, unsaturated carboxylic
Acid, alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, it is described when N- dimethyl-alkyl tertiary amine, the reaction of halogenated cyclic ethers generate thickener
Unsaturated carboxylic acid can be one or more in acrylic acid, butenoic acid or metal acid-salt, and wherein acrylic acid can be straight chain
Acrylic acid can also be the acrylic acid with branch, and butenoic acid can be the butenoic acid of straight chain, can also be the fourth with branch
Olefin(e) acid, atomic number of alkyl carbon can be 7,8 or 12 in the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the alkyl phenol polyoxy alkene
Polyoxyalkylene ethers can be polyoxyethylene ether or polyethenoxy ether, the alkyl phenol Polyoxyalkylene ethers unsaturated acids in ether unsaturated acid ester
Unsaturated acid ester can be acrylate or butenoate in ester, and wherein acrylate can be the acrylate of straight chain, may be used also
Think that the acrylate with branch, butenoate can be the butenoate of straight chain, can also be the butenoic acid with branch
Ester；Atomic number of alkyl carbon is alkyl in 6-18, such as N, N- dimethyl-alkyl tertiary amine in the N, N- dimethyl-alkyl tertiary amine
Carbon atom number can be 8,9 or 12；Halo groups are fluorine, chlorine or bromine in the halogenated cyclic ethers, such as can be fluoro cyclic ethers, can
Think chloro cyclic ethers, can also be bromo cyclic ethers, suitable unsaturated carboxylic acid, alkyl phenol polyoxy are chosen with specific reference to practical application
Alkene ether unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine, halogenated cyclic ethers generate thickener.
In fracturing fluid thickener preparation method provided by the invention, the addition N, N- dimethyl-alkyl tertiary amine and halogenated
The fracturing fluid thickener is made in cyclic ethers, reaction time 6-8h, including：
The N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers is added, gluey production is made in reaction time 8-10h
Object；
The gum-like product is invaded into bubble in ethanol；
The gum-like product invaded after steeping is rinsed, dried and crushed, the fracturing fluid thickener is made.
The present invention also provides a kind of fracturing fluid, the fracturing fluid includes at least above-mentioned fracturing fluid thickener, fracturing fluid thickening
Agent is one of the main additive in fracturing fluid, and performance quality suffers from weight to fracturing fluid comprehensive performance, pressing crack construction effect
Influence, especially face high temperature, hypotonic, the quick reservoir of alkali exploitation, need thickening capabilities it is stronger, to formation damage smaller, high temperature
The good thickener of stability, in of the invention, when fracturing fluid includes the fracturing fluid thickener of above-mentioned preparation, fracturing fluid thickener is being pressed
Split liquid mass percent can be 0.10%-0.60%, for example, the mass percent of fracturing fluid can be 0.1%,
0.15%, 0.25% or 0.5%, fracturing fluid thickener provided by the invention is by acrylamide, unsaturated carboxylic acid, alkyl phenol
Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine, halogenated cyclic ethers, initiator and water mixing composition, the fracturing fluid increase
Thick dose compared with the thickening agent in the prior art based on guanidine glue and its modifier, fracturing fluid thickener provided by the invention is in water
In rise viscous fast, meet continuous mixture requirement, there is good Efficient Adhesive Promotion, adjust it in due course and realize that drop is blocked water and taken using concentration
Sand liquid function, not corrupt, heat-resistant salt-resistant performance is good, so that the fracturing fluid recovery (backflow) effect is good, it can be achieved that without liquid nitrogen with note item
The quick row of returning under part, returns that drain recovery process is simple, and utilization rate is high, it is only necessary to do simple filtration and handle i.e. reusable, institute
It, can also while environmentally friendly pressure break can be alleviated with the fracturing fluid of the fracturing fluid thickener provided by the invention for containing above-mentioned preparation
It is enough preferably to meet the requirement of " batch production " fracturing work.
Fracturing fluid thickener provided by the invention, by by acrylamide, unsaturated carboxylic acid, alkyl phenol Polyoxyalkylene ethers insatiable hunger
With acid esters, N, N- dimethyl-alkyl tertiary amine, halogenated cyclic ethers, initiator and water are mixed to prepare the fracturing fluid thickener, and described third
Acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and
The sum of mass percent of the halogenated cyclic ethers is 15%~25%, the mass percent of the initiator is 0.04%~
0.09%, when which solves in the prior art using guanidine glue and its modifier as the thickener of fracturing fluid due to
It is big that guanidine glue and its easy corruption of modifier cause to return drain intractability after breaking gel, of high cost, reuses the technology of poor feasibility
Problem；The present invention is easy to operate easily controllable in preparation process by proposing a kind of preparation method of fracturing fluid thickener, prepares
Made of fracturing fluid thickener it is not corrupt, heat-resistant salt-resistant rises viscous fast in water, meets continuous mixture requirement, fracturing fluid thickening
Agent has good Efficient Adhesive Promotion, and adjust it in due course just can realize that drop blocks water and load fluid function using concentration；The present invention also carries
For a kind of fracturing fluid, which includes the fracturing fluid thickener of above-mentioned preparation, and the fracturing fluid returns drain processing work when application
Skill is simple, flowback effect is preferable, cost is relatively low, high recycling rate, can meet " factory very well while alleviating environmentally friendly pressure break
Change " fracturing work requirement.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, shall fall within the protection scope of the present invention.
Fracturing fluid thickener provided by the invention can be added in fracturing fluid, be used for low permeability sandstone reservoirs oil-gas field fracturing
Drop blocks water and load fluid in the process, or is also applied in other petroleum drilling fluids, the viscosity for increasing drilling fluid.
Embodiment 1
In the present embodiment, the raw material of fracturing fluid thickener is constituted and the quality of each ingredient is as follows：
Acrylic acid：18.01g；
Acrylamide：70.37g；
Nonyl phenol polyethenoxy ether acrylate：6.26g；
N, N- dimethyl-hexyl tertiary amine：1.20g；
Fluoro propylene oxide：0.75g
Initiator：0.40g；
Water：386.36g；
Initiator is made of ammonium persulfate and potassium thiosulfate, and the quality of ammonium persulfate and potassium thiosulfate is respectively：
Ammonium persulfate：0.21g；
Potassium thiosulfate：0.19g.
Specific preparation process is as follows：
18.01g acrylic acid is dissolved in 386.36g water, is 7 with potassium hydroxide adjustment pH, water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, the acrylamide and 6.26g nonylphenol polyoxyethylene ether propylene of 70.37g is added
Acid esters stirring and dissolving；
It is separately added into 0.21g ammonium persulfates and 0.19g potassium thiosulfates, after reacting 1h, adds 1.20gN, N- diformazans
Base-hexyl tertiary amine and 0.75g fluoro propylene oxide, reaction are made gum-like product after 8-10 hours, bubble glue are invaded with a large amount of ethyl alcohol
Then shape product rinses, fracturing fluid thickener of the present invention is made in dries pulverizing.
The fracturing fluid thickener prepared in embodiment 1 is detected, each performance parameter for obtaining fracturing fluid thickener is：
Degree of hydrolysis：11.5%；Intrinsic viscosity：787.7ml/g；Viscosity average molecular weigh：334.68×104g/mol。
Fracturing fluid thickener provided by the invention is not corrupt, heat-resistant salt-resistant better performances, rises glue soon in water, meets continuous
Mixture requirement, has good Efficient Adhesive Promotion, solves in the prior art using guanidine glue and its modifier as the thickening of fracturing fluid
It is of high cost since to cause to return drain intractability after breaking gel big for guanidine glue and its easy corruption of modifier when agent, reuse feasibility
The technical problem of difference, fracturing fluid thickener prepared by the present invention are added in fracturing fluid, and the fracturing fluid recovery (backflow) effect of formation is good, can
It realizes without liquid nitrogen with the quick row of returning under the conditions of note.And it is simple to return drain recovery process, and utilization rate is high, it is only necessary to do simple filtration
Processing is i.e. reusable, can also meet the requirement of " batch production " fracturing work while capable of alleviating environmentally friendly pressure break very well.
Embodiment 2
In the present embodiment, the raw material of fracturing fluid thickener is constituted and the quality of each ingredient is as follows：
Acrylic acid：18.01g；
Acrylamide：70.37g；
Octyl phenol polyoxyethylene ether acrylate：6.40g；
N, N- dimethyl-octyl tertiary amine：1.46g；
Polychlorinated dibenzo-furans：0.92g
Initiator：0.25g；
Water：388.64g；
Initiator is made of ammonium persulfate and potassium thiosulfate, and the quality of ammonium persulfate and potassium thiosulfate is respectively：
Ammonium persulfate：0.136g；
Potassium thiosulfate：0.114g.
Specific preparation process is as follows：
18.01g acrylic acid is dissolved in 388.64g water, is 7 with potassium hydroxide adjustment pH, water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, the acrylamide and 6.40g octyl phenol polyoxyethylene ether acrylic acid of 70.37g is added
Ester stirring and dissolving；
It is separately added into 0.136g ammonium persulfates and 0.114g potassium thiosulfates, after reacting 1h, adds 1.46gN, N- diformazans
Base-octyl tertiary amine and 0.92g polychlorinated dibenzo-furans, reaction are made gum-like product after 8-10 hours, bubble glue are invaded with a large amount of ethyl alcohol
Then shape product rinses, fracturing fluid thickener of the present invention is made in dries pulverizing.
The fracturing fluid thickener prepared in embodiment 2 is detected, each performance parameter for obtaining fracturing fluid thickener is：
Degree of hydrolysis：11.1%；Intrinsic viscosity：714.63ml/g；Viscosity average molecular weigh：298.68×104g/mol。
Fracturing fluid thickener provided by the invention is not corrupt, heat-resistant salt-resistant better performances, rises glue soon in water, meets continuous
Mixture requirement, has good Efficient Adhesive Promotion, solves in the prior art using guanidine glue and its modifier as the thickening of fracturing fluid
It is of high cost since to cause to return drain intractability after breaking gel big for guanidine glue and its easy corruption of modifier when agent, reuse feasibility
The technical problem of difference, fracturing fluid thickener prepared by the present invention are added in fracturing fluid, and the fracturing fluid recovery (backflow) effect of formation is good, can
It realizes without liquid nitrogen with the quick row of returning under the conditions of note.And it is simple to return drain recovery process, and utilization rate is high, it is only necessary to do simple filtration
Processing is i.e. reusable, can also meet the requirement of " batch production " fracturing work while capable of alleviating environmentally friendly pressure break very well.
Embodiment 3
In the present embodiment, the raw material of fracturing fluid thickener is constituted and the quality of each ingredient is as follows：
Butenoic acid：21.52g；
Acrylamide：70.37g；
Dodecyl phenol polyethenoxy ether acrylate：6.68g；
N, N- dimethyl-dodecylamine base tertiary amine：1.86g；
Polychlorinated dibenzo-furans：0.92g；
Initiator：0.40g；
Water：304.05g；
Initiator is made of ammonium persulfate and potassium thiosulfate, and the quality of ammonium persulfate and potassium thiosulfate is respectively：
Ammonium persulfate：0.21g；
Potassium thiosulfate：0.19g.
Specific preparation process is as follows：
21.52g butenoic acids are dissolved in 304.05g water, are 7 with potassium hydroxide adjustment pH, water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, the acrylamide and 6.68g dodecyl phenol polyethenoxy ethers of 70.37g is added
Acrylate stirring and dissolving；
It is separately added into 0.21g ammonium persulfates and 0.19g potassium thiosulfates, after reacting 1h, adds 1.86gN, N- diformazans
Base-dodecyl tertiary amine and 0.92g polychlorinated dibenzo-furans, reaction are made gum-like product after 8-10 hours, are invaded with a large amount of ethyl alcohol
Gum-like product is steeped, is then rinsed, fracturing fluid thickener of the present invention is made in dries pulverizing.
The fracturing fluid thickener prepared in embodiment 3 is detected, each performance parameter for obtaining fracturing fluid thickener is：
Degree of hydrolysis：11.7%；Intrinsic viscosity：728.77ml/g；Viscosity average molecular weigh：320.36×104g/mol。
Fracturing fluid thickener provided by the invention is not corrupt, heat-resistant salt-resistant better performances, rises glue soon in water, meets continuous
Mixture requirement, has good Efficient Adhesive Promotion, solves in the prior art using guanidine glue and its modifier as the thickening of fracturing fluid
It is of high cost since to cause to return drain intractability after breaking gel big for guanidine glue and its easy corruption of modifier when agent, reuse feasibility
The technical problem of difference, fracturing fluid thickener prepared by the present invention are added in fracturing fluid, and the fracturing fluid recovery (backflow) effect of formation is good, can
It realizes without liquid nitrogen with the quick row of returning under the conditions of note.And it is simple to return drain recovery process, and utilization rate is high, it is only necessary to do simple filtration
Processing is i.e. reusable, can also meet the requirement of " batch production " fracturing work while capable of alleviating environmentally friendly pressure break very well.
Embodiment 4
In the present embodiment, the raw material of fracturing fluid thickener is constituted and the quality of each ingredient is as follows：
Butenoic acid：21.52g；
Acrylamide：70.37g；
Nonyl phenol poly-oxypropylene ether butenoate：6.54g；
N, N- dimethyl-dodecylamine base tertiary amine：6.68g；
4- Brominated Epoxy butane：2.30g；
Initiator：0.25g；
Water：429.64g；
And initiator is made of ammonium persulfate and potassium thiosulfate, the quality of ammonium persulfate and potassium thiosulfate is respectively：
Ammonium persulfate：0.136g；
Potassium thiosulfate：0.114g.
Specific preparation process is as follows：
21.52g butenoic acids are dissolved in 429.64g water, are 7 with potassium hydroxide adjustment pH, water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, the acrylamide and 6.54g nonyl phenol poly-oxypropylene ether butylene of 70.37g is added
Acid esters stirring and dissolving；
It is separately added into 0.136g ammonium persulfates and 0.114g potassium thiosulfates, after reacting 1h, adds 6.68gN, N- diformazans
Base-dodecyl tertiary amine and 2.30g 4- Brominated Epoxy butane, gum-like product is made after 8-10 hours in reaction, with a large amount of ethyl alcohol
Bubble gum-like product is invaded, is then rinsed, fracturing fluid thickener of the present invention is made in dries pulverizing.
The fracturing fluid thickener prepared in embodiment 4 is detected, each performance parameter for obtaining fracturing fluid thickener is：
Degree of hydrolysis：11.7%；Intrinsic viscosity：739.68ml/g；Viscosity average molecular weigh：319.68×104g/mol。
Fracturing fluid thickener provided by the invention is not corrupt, heat-resistant salt-resistant better performances, rises glue soon in water, meets continuous
Mixture requirement, there is good Efficient Adhesive Promotion, fracturing fluid thickener prepared by the present invention to be added in fracturing fluid, the pressure break of formation
Liquid flowback effect is good, it can be achieved that without liquid nitrogen with the quick row of returning under the conditions of note.And it is simple to return drain recovery process, and utilization rate is high,
It is i.e. reusable only to need to do simple filtration processing, " batch production " pressure can also be met while environmentally friendly pressure break can be alleviated very well
Split job requirements.
Embodiment 5
In the present embodiment, the raw material of fracturing fluid thickener is constituted and the quality of each ingredient is as follows：
Butenoic acid：21.52g；
Acrylamide：70.37g；
Dodecyl phenol polyethenoxy ether acrylate：6.68g；
N, N- dimethyl-nonyl tertiary amine：1.59g；
4- chloro epoxy butanes：1.06g；
Initiator：0.40g；
Water：404.88g；
And initiator is made of ammonium persulfate and potassium thiosulfate, the quality of ammonium persulfate and potassium thiosulfate is respectively：
Ammonium persulfate：0.21g；
Potassium thiosulfate：0.19g.
Specific preparation process is as follows：
21.52g butenoic acids are dissolved in 404.88g water, are 7 with potassium hydroxide adjustment pH, water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, the acrylamide and 6.68g dodecyl phenol polyethenoxy ethers of 70.37g is added
Acrylate stirring and dissolving；
It is separately added into 0.21g ammonium persulfates and 0.19g potassium thiosulfates, after reacting 1h, adds 1.59g N, N- diformazans
Base-nonyl tertiary amine and 1.06g 4- chloro epoxy butanes, reaction are made gum-like product after 8-10 hours, bubble are invaded with a large amount of ethyl alcohol
Then gum-like product rinses, fracturing fluid thickener of the present invention is made in dries pulverizing.
The fracturing fluid thickener prepared in embodiment 1 is detected, each performance parameter for obtaining fracturing fluid thickener is：
Degree of hydrolysis：11.3%；Intrinsic viscosity：728.94ml/g；Viscosity average molecular weigh：324.69×104g/mol。
Fracturing fluid thickener provided by the invention is not corrupt, heat-resistant salt-resistant better performances, rises glue soon in water, meets continuous
Mixture requirement, there is good Efficient Adhesive Promotion, fracturing fluid thickener prepared by the present invention to be added in fracturing fluid, the pressure break of formation
Liquid flowback effect is good, it can be achieved that without liquid nitrogen with the quick row of returning under the conditions of note, and it is simple to return drain recovery process, utilization rate height,
It is i.e. reusable only to need to do simple filtration processing, " batch production " pressure can also be met while environmentally friendly pressure break can be alleviated very well
Split job requirements.
Embodiment 6
In the present embodiment, the raw material of fracturing fluid thickener is constituted and the quality of each ingredient is as follows：
Butenoic acid：21.52g；
Acrylamide：70.37g；
Dodecylphenol polyethenoxy ether butenoate：6.96g；
N, N- dimethyl-cetyl tertiary amine：2.57g；
Bromopropylene oxide：1.44g；
Initiator：0.25g；
Water：411.44g；
And initiator is made of ammonium persulfate and potassium thiosulfate, the quality of ammonium persulfate and potassium thiosulfate is respectively：
Ammonium persulfate：0.136g；
Potassium thiosulfate：0.114g.
Specific preparation process is as follows：
21.52g butenoic acids are dissolved in 411.44g water, are 7 with potassium hydroxide adjustment pH, water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, the acrylamide and 6.96g dodecylphenol polyethenoxy ethers of 70.37g is added
Butenoate stirring and dissolving；
It is separately added into 0.136g ammonium persulfates and 0.114g potassium thiosulfates, after reacting 1h, adds 2.57g N, N- bis-
Methyl-cetyl tertiary amine and 1.44g bromopropylene oxides, gum-like product is made after 8-10 hours in reaction, with a large amount of ethyl alcohol
Bubble gum-like product is invaded, is then rinsed, fracturing fluid thickener of the present invention is made in dries pulverizing.
The fracturing fluid thickener prepared in embodiment 1 is detected, each performance parameter for obtaining fracturing fluid thickener is：
Degree of hydrolysis：11.4%；Intrinsic viscosity：747.28ml/g；Viscosity average molecular weigh：294.38×104g/mol。
Fracturing fluid thickener provided by the invention is not corrupt, heat-resistant salt-resistant better performances, rises glue soon in water, meets continuous
Mixture requirement, there is good Efficient Adhesive Promotion, fracturing fluid thickener prepared by the present invention to be added in fracturing fluid, the pressure break of formation
Liquid flowback effect is good, it can be achieved that without liquid nitrogen with the quick row of returning under the conditions of note.And it is simple to return drain recovery process, and utilization rate is high,
It is i.e. reusable only to need to do simple filtration processing, " batch production " pressure can also be met while environmentally friendly pressure break can be alleviated very well
Split job requirements.
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of fracturing fluid thickener, which is characterized in that the raw material group of the fracturing fluid thickener becomes：Acrylamide, insatiable hunger
With carboxylic acid, alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, N, N- dimethyl-alkyl tertiary amine, halogenated cyclic ethers, initiator and water, wherein
The acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl
The sum of mass percent of tertiary amine and the halogenated cyclic ethers is 15%~25%, and the mass percent of the initiator is 0.04%
~0.09%；
The acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-
The molar ratio of alkyl tertiary amine and the halogenated cyclic ethers is 99：25：1：1：1；
Unsaturated acid ester is acrylate or butenoate in the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester；
The halogenated cyclic ethers is fluoro propylene oxide, polychlorinated dibenzo-furans, 4- Brominated Epoxies butane, 4- chloros epoxy butane or bromine
For propylene oxide.
2. fracturing fluid thickener according to claim 1, which is characterized in that the initiator is by ammonium persulfate and thio sulphur
Sour potassium composition, and the molar ratio of the ammonium sulfate and the potassium thiosulfate is 1：1.
3. fracturing fluid thickener according to claim 1, which is characterized in that the unsaturated carboxylic acid is acrylic acid, butylene
One or both of acid；
Atomic number of alkyl carbon is 6-18 in the N, N- dimethyl-alkyl tertiary amine.
4. according to any fracturing fluid thickeners of claim 1-3, which is characterized in that the alkyl phenol Polyoxyalkylene ethers insatiable hunger
It is 7,8 or 12 with atomic number of alkyl carbon in acid esters, and Polyoxyalkylene ethers are polyoxy in the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester
Vinethene or polyethenoxy ether.
5. the preparation method of claim 1-4 any one of them fracturing fluid thickeners, which is characterized in that including following procedure：
Unsaturated carboxylic acid is dissolved in water, adjustment pH is 7, and water bath with thermostatic control is to 15 DEG C；
Under conditions of maintaining nitrogen purge, acrylamide and alkyl phenol Polyoxyalkylene ethers unsaturated acid ester stirring and dissolving is added；
Initiator is added, N, N- dimethyl-alkyl tertiary amine and halogenated cyclic ethers is added after reacting 1h, reaction time 6-8h is made
The fracturing fluid thickener, wherein
The acrylamide, the unsaturated carboxylic acid, the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-
The sum of mass percent of alkyl tertiary amine and the halogenated cyclic ethers is 15%~25%, and the initiator quality percentage is
0.04%~0.09%, surplus is water.
6. preparation method according to claim 5, which is characterized in that the acrylamide, the unsaturated carboxylic acid, described
The molar ratio of alkyl phenol Polyoxyalkylene ethers unsaturated acid ester, the N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers is 99：
25：1：1：1；
The initiator is made of ammonium persulfate and potassium thiosulfate, and the molar ratio of the ammonium sulfate and the potassium thiosulfate
It is 1：1.
7. preparation method according to claim 5, which is characterized in that the unsaturated carboxylic acid is in acrylic acid, butenoic acid
One or two；
Atomic number of alkyl carbon is 6-18 in the N, N- dimethyl-alkyl tertiary amine.
8. according to any preparation methods of claim 5-7, which is characterized in that the alkyl phenol Polyoxyalkylene ethers unsaturated acids
Atomic number of alkyl carbon is 7,8 or 12 in ester, and Polyoxyalkylene ethers are polyoxyethylene in the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester
Ether or polyethenoxy ether, unsaturated acid ester is acrylate or butenoic acid in the alkyl phenol Polyoxyalkylene ethers unsaturated acid ester
Ester.
9. according to any preparation methods of claim 5-7, which is characterized in that the addition N, N- dimethyl-alkyl tert
The fracturing fluid thickener is made in amine and halogenated cyclic ethers, reaction time 6-8h, including：
The N, N- dimethyl-alkyl tertiary amine and the halogenated cyclic ethers is added, gum-like product is made in reaction time 8-10h；
The gum-like product is invaded into bubble in ethanol；
The gum-like product invaded after steeping is rinsed, dried and crushed, the fracturing fluid thickener is made.
10. a kind of fracturing fluid, which is characterized in that the fracturing fluid includes at least claim 1-4 any one of them fracturing fluids
Thickener, and mass percent of the fracturing fluid thickener in the fracturing fluid is 0.10%-0.60%.
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| CN101081976A (en) * | 2006-05-29 | 2007-12-05 | 中国科学技术大学 | Fire-resistant non-injury fracturing fluid thickening agent and preparation method and usage thereof |
| CN101945971A (en) * | 2007-12-21 | 2011-01-12 | 3M创新有限公司 | Utilize the method for fluorinated polymer compositions-treated hydrocarbon containing formation |
| CN102858883A (en) * | 2010-02-12 | 2013-01-02 | 罗地亚管理公司 | Rheology Modifier Compositions And Methods Of Use |
| CN103087699A (en) * | 2012-12-27 | 2013-05-08 | 中国石油化工股份有限公司 | Sand-carrying profile control agent composition of fracture-cave type oil deposit and profile control method of profile control agent |
| CN103254887A (en) * | 2013-06-09 | 2013-08-21 | 郑建立 | Anti-drag aqueous fracturing fluid preparation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081976A (en) * | 2006-05-29 | 2007-12-05 | 中国科学技术大学 | Fire-resistant non-injury fracturing fluid thickening agent and preparation method and usage thereof |
| CN101945971A (en) * | 2007-12-21 | 2011-01-12 | 3M创新有限公司 | Utilize the method for fluorinated polymer compositions-treated hydrocarbon containing formation |
| CN102858883A (en) * | 2010-02-12 | 2013-01-02 | 罗地亚管理公司 | Rheology Modifier Compositions And Methods Of Use |
| CN103087699A (en) * | 2012-12-27 | 2013-05-08 | 中国石油化工股份有限公司 | Sand-carrying profile control agent composition of fracture-cave type oil deposit and profile control method of profile control agent |
| CN103254887A (en) * | 2013-06-09 | 2013-08-21 | 郑建立 | Anti-drag aqueous fracturing fluid preparation |
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